CN103964737A - Nano-silicon-modified double-component wear-resistant penetration hardener and preparation method thereof - Google Patents
Nano-silicon-modified double-component wear-resistant penetration hardener and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of protection treatment of concrete materials, and aims to provide a nano-silicon-modified double-component wear-resistant penetration hardener and a preparation method thereof. The hardener comprises a component A and a component B, wherein the component A is composed of silicone prepolymer, a wear-resistant modification material, a stabilizer and a solvent; the component B is composed of a catalyst and a solvent; both components adopt alcohol as the solvent. The nano-silicon-modified double-component wear-resistant penetration hardener provided by the invention has a higher hardening speed and a more obvious wear-resistant effect compared with an aqueous silicate penetration hardener, is stored separately in the form of the component A and the component B to provide better storage stability compared with a single-component organosilicon resin penetration hardener so as to better ensure the permeability to the concrete during use, and adopts nano-silicon sol as the wear-resistant modifier to greatly improve the wearing-resistance of concrete treated by the penetration hardener.
Description
Technical field
The invention belongs to the protective treatment technical field of concrete material, be specifically related to wear-resisting infiltration stiffening agent of a kind of nano-silicon modified double components and preparation method thereof.
Background technology
Along with the development of economy, technology, concrete has been widely applied to the every field of mankind's activity, becomes the foundation stone of social development.And so, normal concrete, when as terrace and pavement usage, also exists and wears no resistance, has been easy to the problems such as ash, dusting.These problems just feature of concrete itself determine: concrete is from being poured into setting and hardening process, and coarse aggregate sinks, grout floating, causes concrete surface to wear no resistance; Moisture content unnecessary after hydration reaction distributes from inside, causes concrete structure mesoporosity many, and degree of compactness is poor.Extraneous corrosive medium as sour gas etc., easily reacts by hole and concrete, and the structural material of corrosion concrete, or reinforcing bar in corrosion concrete structure, cause that concrete expansion ftractures, and has a strong impact on the security of concrete structure.
At present, the technology that improves concrete abrasion-resistant mainly contains three classes, and the first kind is to lay one deck wearing layer at concrete surface.The high-abrasive materials such as wearing layer can ceramic tile, stone material, but exist, cost is high, construction trouble, floor level changes the problems such as larger, thereby the scope of application is few.Equations of The Second Kind is at coating such as concrete surface epoxy resin coating, carbamide resins.Although have certain wear resistance to improve, coating can not improve concrete intensity, and organic coating film is blocked concrete surface hole completely, cause internal steam freely not discharge, easily cause the film delamination of flaking, in addition, organic coating film is shorter work-ing life, and maintenance cost is high.The 3rd class is to use concrete infiltration stiffening agent.Thereby concrete infiltration stiffening agent is a class can infiltrate concrete pore and react with it and strengthen concrete material.Since there is aqueous silicic acid salt penetration stiffening agent from twentieth century, such technology is developed rapidly.
Aqueous silicic acid salt infiltration stiffening agent comprises aqueous silicic acid sodium, potassium silicate, Magnesium Silicate q-agent, lithium silicate etc., due to preparation and constructional method simple, concrete is had to the effect of good enhancing, Hardening, raising wear resistance, on the terraces such as the large supermarket of the countries such as America and Europe, factory, school, airport, applied decades.But the water-based stiffening agents such as water glass, potassium silicate, Magnesium Silicate q-agent, owing to containing the strong basicity such as sodium, potassium metallic element, pH value, often in 12 left and right, easily forms alkaline matter, salts substances etc. at concrete surface and separates out, and not only affects ground apparent, and cause ground to send out cunning, have a strong impact on use.Although aqueous silicic acid lithium stiffening agent " accumulation of salt in the surface soil " problem is few, but still there is slow (often wanting some months later just to there will be obvious gloss and hardness) of setting rate, and mainly by import, causing price high, product shoddy phenomenon in domestic market is of common occurrence.
Prepare the existing more report of patent of invention of aqueous silicate stiffening agent with aqueous silicate and other function components.CN200910055825.2 discloses taking lithium silicate as major ingredient, and magnesium silicofluoride, silane emulsion, Emulsion acrylic resin, paraffin and water are the stiffening agent preparation method of the second component.Using method is to brush the second component after the first component uses and is dried again.This patented technology is mainly utilized lithium silicate and concrete reaction, plays enhancement.Magnesium silicofluoride, silane emulsion play certain hydrophobic interaction, and Emulsion acrylic resin, paraffin play brightening agent effect.The method exists lithium silicate Hardening speed of response slow, and the brightening agent validity period such as paraffin are shorter, and the miscible effect of various ingredients is bad and occur the problems such as muddy.CN201010543000.8 discloses and has utilized nano silicone colloidal sol to be penetrated in concrete pore, under potassium metaaluminate katalysis, reacts with calcium hydroxide and unhydrated cement, generates the gel of crosslinking structure.The organosilicon that another key ingredient potassium methyl silicate is hydrophobic nature, forms one deck hydrophobic film at concrete surface, reaches dustproof, refuses water effect.The shortcoming existing is mainly that the reaction of silicon sol and calcium hydroxide is slow, and the cross-linking density of the gel of generation is little, and to concrete Hardening DeGrain, wear resisting property does not obviously promote.Thereafter disclosed CN201110354668.2 and CN201110152386.4, crucial composition is all identical with CN201010543000.8 with preparation thinking.The disclosed a kind of concrete curing sealing agent for low-temperature cold store of CN201110405075.4, it prepares thinking is that lithium, titanium, silicon-dioxide and water react under heating condition, generates aqueous lithium based stiffening agent.Except the slower shortcoming of aqueous lithium based stiffening agent and concrete reaction, also there is the problem in the preparation methods such as lithium and water reaction are violent, and security is low.CN201110083155.2 discloses a kind of multifunctional concrete structure durability protective agent and methods for making and using same thereof, and its component is: with/without the compound fluorine siloxane-acrylate copolymer of machine, lithium silicate, water glass, lithium molybdate, sodium tetraborate, sodium sulfate, phenylpropyl alcohol triazole, nano titanium oxide, dehydrated alcohol and water.Concrete and inner reinforcing bar are protected although many-sided, the statement that concrete abrasion-resistant performance does not improve.
Due to organosilicon preferably penetrating quality, good hydrophobic function on concrete, concrete is had to certain provide protection, be the more class Concrete Protective Agent of research in recent years.And simple organosilane or organic silane low polymer, although also can penetrate in concrete, play certain protective effect, but its protective mechanism is mainly to utilize the hydrophobic interaction of silane at concrete surface, and because its polymerization degree is low, often can not form the network-like macromole of crosslinked shape, thereby the filling to concrete pore and enhancement are very weak, more there is no the raising on wear resisting property.Have and as disclosedly in CN200910027824.7 obtain silane low polymer with the alkenyl alkoxy silane polymerization that contains unsaturated double-bond; although good penetrability, water-intake rate are low; weather resistance to concrete structure has provide protection, but does not mention concrete is had to enhancement.Silane prepolymer particularly contains the network-like macromole gel that trifunctional chains or the siloxane prepolymer of four senses link generates after hydrolytic-polymeric reaction, hole in can air free concrete, by the control of monomer structure, proportioning, effect transparent, that hardness is high, glossiness is high, hardness is high that the macromolecular resin of its complete polycondensation can reach, thereby fine is played closed concrete hole, strengthen concrete effect.The disclosed technical scheme of CN200910186739.5 adopts this kind of thinking exactly.The liquid composition of preparation strengthens Hardening successful to concrete surface layer, prevents in addition that dusting from playing the effects such as dirt simultaneously.But, owing to containing hydrochloric acid in the silane prepolymer liquid after the hydrolysis of silane and tetrachloro silicane, cause the poor storage stability of silane pre-polymer, easily further hydrolytic polymerization before use, cause liquid thickening or gel, affected the penetrating quality on concrete or directly can not use.And taking silicone resin as Hardening material, wear resistance does not reach service requirements merely.
Summary of the invention
The technical problem to be solved in the present invention is, overcome in prior art aqueous silicic acid salt infiltration stiffening agent onset time long, wear-resisting effect not, the easy problem such as weak, the single-component silicone resin class infiltration stiffening agent poor storage stability wear resistance shortcoming of " accumulation of salt in the surface soil ", silicane treatment agent reinforced effects, wear-resisting infiltration stiffening agent of a kind of nano-silicon modified double components and preparation method thereof is provided.
For technical solution problem, solution of the present invention is:
Provide a kind of nano-silicon modified double components wear-resisting infiltration stiffening agent, this stiffening agent comprises two kinds of components of first, second, wherein:
(1) first component is by siloxane prepolymer, wear-resisting material modified, stablizer and solvent composition; The ratio that siloxane prepolymer accounts for total mass is 15~40%, and the wear-resisting material modified total mass ratio that accounts for is 1.7~34.95%, and it is 0.1~3% that stablizer accounts for total mass ratio, and all the other are solvent;
Described siloxane prepolymer refers to, by be hydrolyzed in solvent prepolymerization or by least one the silane prepolymer prepared by being hydrolyzed prepolymerization with the siloxanes (A3) of two senses link in the siloxanes (A1) that contains four senses links or the siloxanes (A2) that contains trifunctional link of at least one in the siloxanes (A1) that contains four senses links or the siloxanes (A2) that contains trifunctional link;
Siloxanes (A1), the siloxanes (A2) that contains trifunctional link that contains four sense links, the siloxanes (A3) that contains two sense links are respectively by following various expression:
In formula, R1~R4, R6~R8, R10 and R12 are the alkyl or phenyl of 1~12 carbon; R5, R9, R11 are the alkyl or phenyl of H or 1~12 carbon;
Described wear-resisting material modified be nano silicon;
Described stablizer is the polyol of small molecules amount, is the one in following compound: trolamine, diethanolamine, glycerol, tetramethylolmethane, Macrogol 200 or poly(oxyethylene glycol) 400;
(2) component B is made up of catalysts and solvents, and catalyzer: the mass ratio of solvent is 1~10: 90~99;
Described catalyzer is organic tin, is the one in following compound: dibutyltin diacetate, dibutyl tin laurate, two sad dibutyl tins or two sad tin ethides;
Described in two kinds of components of first, second, solvent is ethanol.
In the present invention, described nano silicon is to provide with the form of nano silicon dioxide sol, and in colloidal sol, the particle diameter of silicon-dioxide is 20~100nm, and pH is 3~7, and mass concentration is 10~50%.
The present invention further provides the method for preparing the wear-resisting infiltration stiffening agent of aforementioned nano-silicon modified double components, comprised respectively the preparation process of two kinds of components of first, second:
(1) preparation method of first component comprises siloxanes pre-polymerization and two steps of wear-resisting modification:
Siloxanes pre-polymerization:
At least one in the siloxanes (A2) that the siloxanes (A1) that contains four sense links, trifunctional are chained, or at least one in the siloxanes (A2) of the siloxanes (A1) of four senses links, trifunctional link added in alcohol solvent with the siloxanes (A3) that two senses chain, and prepolymerization is hydrolyzed under ion-exchange resin catalyzed; After prepolymerization completes, filtered and recycled ion exchange resin, steams part ethanol and unreacted water, and to be deployed into mass concentration with ethanol be 50% siloxane prepolymer solution; Wherein, siloxanes: water: ethanol: the mass ratio of ion exchange resin is 20~80: 10~40: 7~40: 1~3, being hydrolyzed prepolymerized temperature of reaction is 30~80 DEG C, the reaction times is 2~8h;
Wear-resisting modification:
According to siloxane prepolymer solution: nano silicon dioxide sol: the mass ratio of stablizer is: 30~80: 17~69.9: 0.1~3, in the siloxane prepolymer solution that is 50% to mass concentration, add successively stablizer, nano silicon dioxide sol, stir and obtain first component;
(2) preparation method of component B:
According to catalyzer: the mass ratio of ethanol is 1~10: 90~99, by catalyzer and the ethanol component B that at room temperature stirs to obtain.
As preferred version, the ion exchange resin using in the step of described siloxanes pre-polymerization is cationic ion exchange resin.
As further preferred version, the ion exchange resin using in the step of described siloxanes pre-polymerization is strongly acidic styrene type cation exchange resin.
As further preferred version, the ion exchange resin using in the step of described siloxanes pre-polymerization is 732# Zeo-karb.
Prior art scheme relatively, advantage of the present invention is:
1, technical scheme of the present invention provides a kind of than the wear-resisting infiltration stiffening agent of aqueous silicic acid salt infiltration stiffening agent Hardening speed nano-silicon modified double components fast, wear-resisting successful.Its first component is at least one in the siloxanes of the siloxanes that contains four-functional group link and trifunctional link, or the siloxanes of four-functional group link and trifunctional chain the prepolymer that the siloxanes of at least one and two functional groups link forms through hydrolysis.Second component is catalyzer.When the first and second components are mixed and are applied to after concrete, the moisture generation hydrolysis reaction in stiffening agent and concrete, continues polymerization reaction take place between prepolymer molecule, meanwhile, prepolymer also with concrete in-there is condensation reaction in OH.The final silicone resin with spatial network shape structure that forms, by kind and the proportioning control of siloxanes, the performances such as the hardness of silicone resin, glossiness, hydrophobicity are outstanding, simultaneously, in first component, also have the sol-gel modified component of inorganic silicon dioxide nano, its Nano Particle and colloidal sol form, realized the enhancing modified of silicon-dioxide to silicone resin well, make the stiffening agent appearance transparent after nanometer grade silica is uniformly dispersed, solidifies colourless, do not affect appearance effect.
2, technical scheme provided by the invention is two component storages, silicone resin type infiltration stiffening agent than single component has better storage stability, more can ensure to use time to concrete perviousness, and, the present invention uses Nano silica sol as wear-resisting properties-correcting agent, and after making to process, concrete wear resistance improves greatly.
Brief description of the drawings
Fig. 1 is the TEM figure of the wear-resisting infiltration stiffening agent of nano-silicon modified double components liquid;
Fig. 2 is the SEM figure of film after the wear-resisting infiltration stiffening agent of nano-silicon modified double components liquid curing film forming.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Should be understood that these embodiment are for the present invention being described instead of limiting the scope of the invention.In embodiment, not marked implementation condition is generally the condition in normal experiment.
The preparation method of the wear-resisting infiltration stiffening agent of nano-silicon modified double components of the present invention, comprises respectively the preparation process of two kinds of components of first, second:
(1) preparation method of first component comprises siloxanes pre-polymerization and two steps of wear-resisting modification:
Siloxanes pre-polymerization:
At least one in the siloxanes (A2) that the siloxanes (A1) that contains four sense links, trifunctional are chained, or at least one in the siloxanes (A2) of the siloxanes (A1) of four senses links, trifunctional link added in alcohol solvent with the siloxanes (A3) that two senses chain, and prepolymerization is hydrolyzed under ion-exchange resin catalyzed; After prepolymerization completes, filtered and recycled ion exchange resin, steams part ethanol and unreacted water, and to be deployed into mass concentration with ethanol be 50% siloxane prepolymer solution; Wherein, siloxanes: water: ethanol: the mass ratio of ion exchange resin is 20~80: 10~40: 7~40: 1~3, being hydrolyzed prepolymerized temperature of reaction is 30~80 DEG C, the reaction times is 2~8h;
Wear-resisting modification:
According to siloxane prepolymer solution: nano silicon dioxide sol: the mass ratio of stablizer is: 30~80: 17~69.9: 0.1~3, in the siloxane prepolymer solution that is 50% to mass concentration, add successively stablizer, nano silicon dioxide sol, stir and obtain first component;
(2) preparation method of component B:
According to catalyzer: the mass ratio of ethanol is 1~10: 90~99, by catalyzer and the ethanol component B that at room temperature stirs to obtain.
Test parameter in each embodiment sees the following form:
The wear-resisting infiltration stiffening agent of nano-silicon modified double components prepared by the present invention is to cement-base concrete base material wear resisting property
Impact sees the following form, and testing standard is: the method for GB/T19766-2005 appendix A.
Can find out from test result, the wear-resisting infiltration stiffening agent of nano-silicon modified double components prepared by technical solution of the present invention has obvious raising to cement-base concrete base material wear resisting property.
Above-described embodiment is only explanation technical conceive of the present invention and feature, its objective is to allow to be familiar with these those skilled in the art and can to understand content of the present invention enforcement according to this, can not limit the scope of the invention with this.All equivalents that spirit has been done according to the present invention or modification, within all should being encompassed in protection scope of the present invention.
Claims (6)
1. the wear-resisting infiltration stiffening agent of nano-silicon modified double components, is characterized in that, this stiffening agent comprises two kinds of components of first, second, wherein:
(1) first component is by siloxane prepolymer, wear-resisting material modified, stablizer and solvent composition; The ratio that siloxane prepolymer accounts for total mass is 15~40%, and the wear-resisting material modified total mass ratio that accounts for is 1.7~34.95%, and it is 0.1~3% that stablizer accounts for total mass ratio, and all the other are solvent;
Described siloxane prepolymer refers to, by be hydrolyzed in solvent prepolymerization or by least one the silane prepolymer prepared by being hydrolyzed prepolymerization with the siloxanes (A3) of two senses link in the siloxanes (A1) that contains four senses links or the siloxanes (A2) that contains trifunctional link of at least one in the siloxanes (A1) that contains four senses links or the siloxanes (A2) that contains trifunctional link;
Siloxanes (A1), the siloxanes (A2) that contains trifunctional link that contains four sense links, the siloxanes (A3) that contains two sense links are respectively by following various expression:
In formula, R1~R4, R6~R8, R10 and R12 are the alkyl or phenyl of 1~12 carbon; R5, R9, R11 are the alkyl or phenyl of H or 1~12 carbon;
Described wear-resisting material modified be nano silicon;
Described stablizer is the polyol of small molecules amount, is the one in following compound: trolamine, diethanolamine, glycerol, tetramethylolmethane, Macrogol 200 or poly(oxyethylene glycol) 400;
(2) component B is made up of catalysts and solvents, and catalyzer: the mass ratio of solvent is 1~10: 90~99;
Described catalyzer is organic tin, is the one in following compound: dibutyltin diacetate, dibutyl tin laurate, two sad dibutyl tins or two sad tin ethides;
Described in two kinds of components of first, second, solvent is ethanol.
2. the wear-resisting infiltration stiffening agent of nano-silicon modified double components according to claim 1, it is characterized in that, described nano silicon is to provide with the form of nano silicon dioxide sol, and in colloidal sol, the particle diameter of silicon-dioxide is 20~100nm, pH is 3~7, and mass concentration is 10~50%.
3. a method of preparing the wear-resisting infiltration stiffening agent of nano-silicon modified double components described in claim 1, is characterized in that, comprises respectively the preparation process of two kinds of components of first, second:
(1) preparation method of first component comprises siloxanes pre-polymerization and two steps of wear-resisting modification:
Siloxanes pre-polymerization:
At least one in the siloxanes (A2) that the siloxanes (A1) that contains four sense links, trifunctional are chained, or at least one in the siloxanes (A2) of the siloxanes (A1) of four senses links, trifunctional link added in alcohol solvent with the siloxanes (A3) that two senses chain, and prepolymerization is hydrolyzed under ion-exchange resin catalyzed; After prepolymerization completes, filtered and recycled ion exchange resin, steams part ethanol and unreacted water, and to be deployed into mass concentration with ethanol be 50% siloxane prepolymer solution; Wherein, siloxanes: water: ethanol: the mass ratio of ion exchange resin is 20~80: 10~40: 7~40: 1~3, being hydrolyzed prepolymerized temperature of reaction is 30~80 DEG C, the reaction times is 2~8h;
Wear-resisting modification:
According to siloxane prepolymer solution: nano silicon dioxide sol: the mass ratio of stablizer is: 30~80: 17~69.9: 0.1~3, in the siloxane prepolymer solution that is 50% to mass concentration, add successively stablizer, nano silicon dioxide sol, stir and obtain first component;
(2) preparation method of component B:
According to catalyzer: the mass ratio of ethanol is 1~10: 90~99, by catalyzer and the ethanol component B that at room temperature stirs to obtain.
4. method according to claim 3, is characterized in that, the ion exchange resin using in the step of described siloxanes pre-polymerization is cationic ion exchange resin.
5. method according to claim 3, is characterized in that, the ion exchange resin using in the step of described siloxanes pre-polymerization is strongly acidic styrene type cation exchange resin.
6. method according to claim 3, is characterized in that, the ion exchange resin using in the step of described siloxanes pre-polymerization is 732# Zeo-karb.
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